CN108439858A - A kind of preparation method of expansion heat insulation type fire proofing material - Google Patents
A kind of preparation method of expansion heat insulation type fire proofing material Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B26/00—Compositions of mortars, concrete or artificial stone, containing only organic binders, e.g. polymer or resin concrete
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- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/20—Resistance against chemical, physical or biological attack
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Abstract
The invention discloses a kind of preparation methods of expansion heat insulation type fire proofing material, belong to fire proofing material preparing technical field.The bentonite that the present invention adds is after high-temperature calcination,Micro- stomata can be formed inside it and inhibits the burning between particle,Wherein expansiveness graphite can invade in micro- stomata,The modification alumina silicate fibre fusing point on fire proofing material surface is at 1500 DEG C or more,Enhancing protective effect is also functioned to fire proofing material,Fire resisting building stones and graphene are combined closely by Polycarbosilane,It is combined again by silicon carbide after high temperature firing,Since silicon carbide has high bond strength,And silicon carbide after high-temperature oxydation can fire proofing material surface formed one layer it is fine and close,Firm silica membrane,In addition,Silicon carbide can also at high temperature react to form zirconium dioxide silica membrane with zirconium boride,To reduce in pyroprocess because expansion generate to external carbuncle,To improve fire proofing material compression strength in a high temperauture environment,It has a extensive future.
Description
Technical field
The invention discloses a kind of preparation methods of expansion heat insulation type fire proofing material, belong to fire proofing material technology of preparing neck
Domain.
Background technology
Fire proofing material, be added to certain synthetic material with fire performance matrix or inherently with high temperature resistant, it is heat-resisting,
The material of flame-retarding characteristic.The production scale of most enterprises is all little, and technological process automatization level is not high, the formula of many products
Technique is similar, lacks inherent characteristic, and the raw material to being exclusively used in fireproof coating is studied not enough, and shortage is exclusively used in expansion fire-proof
The resin of coating, fireproof coating production and the equipment of construction do not match also, and fireproof coating is applied in engineering, to type kind
Maintenance reparation etc. during selection, the determination of protective layer thickness, the supervision of construction quality, use all be there are problems that.Fire prevention
Plate is the most commonly used currently on the market material, and fire prevention furred ceiling day is installed in building exit channel, stairwell and corridor etc.
Card, people's safe escape when can ensure that fire, and protect invasion of the people from spreading the intensity of a fire.
According to the requirements at the higher level that the similar technique experience of developed countries and China users constantly propose, fire prevention applies
There is also some gaps and problems in the exploitation and application of material.
Present fire resistant doorsets are substantially all in the core material of filling out using perlite series of products as fire resistant doorsets, and perlite is
A kind of nontoxic, tasteless, non-ignitable, material for being stale-proof, the product are mainly used for keeping the temperature, being heat-insulated for building roofing and wall;Building
The aglite of material;Various industrial equipments, pipe insulation layer;The soilless culture of agricultural and gardening, retain water and nutrients etc. are extensive
Applied to industries such as oil, chemical industry, electric power, building, metallurgy.Perlite temperature in use is -256~800 DEG C, and refractory temperature is low,
The fire resistant doorsets produced are allowed to have a long way to go with American-European.This is significant as preventing fires for fire resistant doorsets, therefore the fire resisting of fire resistant doorsets
Temperature and time is extremely important, and in actual life when there is fire generation, the temperature of flame is entirely possible to be more than 1200
DEG C, when temperature be more than 1200 DEG C when, existing fire resistant doorsets be difficult at this temperature for a long time in do not burnt by big fire, after burn-through
Fire resistant doorsets, which just lose, protects this Missions of thousands upon thousands the people's lives and property.Fire proofing material refractory heat-insulating performance at present
Difference is easy fire of leaping up, and expansion multiplying power is low under the high temperature conditions, is not easy to form thermal insulation layer, and can make after fire proofing material expansion
Its compression strength reduces.
Therefore, a kind of expansion heat insulation type fire proofing material of invention has positive effect to fire proofing material preparing technical field.
Invention content
Present invention mainly solves the technical issues of, it is poor for current fire proofing material refractory heat-insulating performance, be easy fire of leaping up, and
Expansion multiplying power is low under the high temperature conditions, is not easy to form thermal insulation layer, and can make the reduction of its compression strength after fire proofing material expansion
Defect provides a kind of preparation method of expansion heat insulation type fire proofing material.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is:
A kind of preparation method of expansion heat insulation type fire proofing material, it is characterised in that specifically preparation process is:
(1)It counts in parts by weight, 70~80 parts of kaolin, 20~30 parts of aluminium oxide, 10~15 is added into 400~500 parts of water
Part titanium dioxide, 20~22 parts of aluminum phosphates, are dispersed with stirring and suspension slurry are made, and phosphoric acid solution is added into suspension slurry and adjusts suspension
The pH of slurries, heat temperature raising, heat preservation obtain mixed serum;
(2)It is sieved after bentonite is ground, high-temperature calcination obtains light-burned bentonite, by 20~30 parts of diatomite, 10~15 parts light
Bentonite mixing is burnt, sieving obtains mixed clay;
(3)35~50 parts of nanometer titanium dioxide silica aerogels, 30~40 parts of above-mentioned mixed clays, 200~300 parts of water are mixed to get
Nanometer titanium dioxide silica aerogel slurries mix mixed serum, nanometer titanium dioxide silica aerogel slurries, and heating obtains melting charge
Liquid obtains modified alumina silicate fibre through spinning;
(4)150~200mL methyl-silicone oils are taken to be added in the three-necked flask with thermometer and reflux, under nitrogen protection
Three-necked flask is moved into sand-bath pot, after insulation reaction, heating continues insulation reaction, after reaction cooled to room temperature,
Obtain product;
(5)200~300mL dimethylbenzene is added into above-mentioned product, is filtered after being stirred, obtains filtrate, filtrate is transferred to rotation
Turn in evaporimeter, concentrated by rotary evaporation obtains concentrate, takes 30~40g zirconium borides to be added in pulverizer and crushes, obtains boronation zirconium powder
Boronation zirconium powder, concentrate, 100~200mL deionized waters are added in beaker, after being stirred, obtain bonding agent by end;
(6)It counts in parts by weight, 40~50 parts of white fused aluminas, 30~40 parts of obsidians, 20~25 parts of expansible graphites is added to
It is poured into sand mixer after being crushed in pulverizer, then 10~15 parts of alumina powders, 0.3~0.5 part of polypropylene is added into sand mixer
Sour sodium, 3~5 parts of zirconium dioxides, 5~8 parts of graphenes, are stirred, and sequentially add 8~10 parts of bonding agents and 20~25 parts change
Property alumina silicate fibre, continue to be stirred, obtain mixing building stones, mixing building stones are packed into modified alumina silicate fibre cladding of tangling
In mold, hot pressing obtains expansion heat insulation type fire proofing material.
Step(1)The mass fraction of the phosphoric acid solution is 20%, and the pH value for adjusting suspension slurry is 5~6, and heating rises
Temperature is 50~60 DEG C after temperature, and soaking time is 10~15h.
Step(2)It is 400 mesh that the bentonite, which grinds be sieved specification, and high-temperature calcination temperature is 600~800 DEG C, is forged
The burning time is 2~4h, and be sieved specification is 400~500 mesh.
Step(3)The mixed serum, nanometer titanium dioxide silica aerogel slurries mixed volume ratio are 4:1, heat temperature raising
Temperature is 700~800 DEG C afterwards.
Step(4)The control sand-bath temperature is 420~430 DEG C, and the insulation reaction time is 1~2h, temperature after heating
It it is 460~480 DEG C, the continuation insulation reaction time is 40~50min.
Step(5)The time that is stirred is 10~15min, and concentrated by rotary evaporation temperature is 80~90 DEG C, concentrated by rotary evaporation
Time is 40~50min, and it is 30~40min that zirconium boride, which is added in pulverizer grinding time, be stirred the time be 15~
20min。
Step(6)Grain diameter is 1~3mm after the crushing, and it is 10~20min to be stirred the time, continues to stir
Incorporation time is 5~10min, and hot pressing time is 30~35min, and control hot pressing pressure is 10~20MPa, hot pressing temperature 200
~300 DEG C.
The beneficial effects of the invention are as follows:
(1)Suspension slurry is made as raw material using kaolin powder, aluminium oxide, titanium dioxide, aluminum phosphate in the present invention, and phosphoric acid is added and adjusts
Mixed serum is obtained after pH, mixed clay is prepared with diatomite and light-burned bentonite, by mixed clay, nano silicon dioxide
Aeroge is mixed to prepare nanometer titanium dioxide silica aerogel slurries, and mixed serum, nanometer titanium dioxide silica aerogel slurries are mixed and are added
Heat fusing obtains melting feed liquid, obtains modified alumina silicate fibre by spinning, methyl-silicone oil is placed under hot conditions and is cracked,
Pyrolysis product is obtained, pyrolysis product is miscible with dimethylbenzene, concentrate is obtained through filtering, rotary evaporation, with boronation zirconium powder, dense
Contracting liquid be raw material bonding agent is prepared, finally by white fused alumina, obsidian crush after with alumina powder, Sodium Polyacrylate, dioxy
Change the mixing of the raw materials such as zirconium, graphene, be put into sand mixer and be mixed, then mix bonding agent and obtain mixing building stones, stone will be mixed
Material is tangled with modified alumina silicate fibre, and cladding is die-filling, and hot pressing obtains expansion heat insulation type fire proofing material, the bentonite that the present invention adds
After high-temperature calcination, inside can form micro- stomata and inhibit the burning between particle, wherein expansiveness graphite can invade
In micro- stomata, after being subjected to high temperature action, since expansible graphite thermal coefficient is big, in the diabatic process of fire proofing material, prevent
The surface of fiery material is rapidly heated, and expanded graphite meeting microdilatancy becomes diastole state from rolled state, improves the outer of fire proofing material
Surface radiating area plays cooling effect to fire proofing material internal layer, and the modification alumina silicate fibre fusing point on fire proofing material surface exists
1500 DEG C or more, enhancing protective effect also functioned to fire proofing material, obsidian used is highly expanded rate volcanic rock, 1000 DEG C with
Expansion rate is up to 5~10 times under upper hot conditions, forms the thermal insulation layer of high thickness;
(2)The present invention is Polycarbosilane with the concentrate prepared by methyl-silicone oil, using Polycarbosilane and zirconium boride as bonding agent,
Polycarbosilane can be cracked into silicon carbide whisker at high temperature in fire proofing material, and silicon carbide whisker, which is filled in fire proofing material, to be reduced
Stomata improves the compression strength when high temperature of fire proofing material, and fire resisting building stones and graphene are combined closely by Polycarbosilane, then are passed through
It is combined by silicon carbide after high temperature firing, since silicon carbide has high bond strength, and silicon carbide is after high-temperature oxydation
One layer of fine and close, firm silica membrane can be formed on fire proofing material surface, in addition, silicon carbide can also be with zirconium boride in height
The lower reaction of temperature forms zirconia-silica film, to further increase the compressive resistance of fire proofing material at high temperature, adds
The graphene and expansible graphite entered can make fire proofing material after by high-temperature expansion interior contact it is even closer, to reduce high temperature mistake
Because what expansion generated has a extensive future to external carbuncle to improve fire proofing material compression strength in a high temperauture environment in journey.
Specific implementation mode
It counts in parts by weight, 70~80 parts of kaolin, 20~30 parts of aluminium oxide, 10~15 parts of titaniums is added into 400~500 parts of water
White powder, 20~22 parts of aluminum phosphates, are dispersed with stirring and suspension slurry are made, and the phosphoric acid that mass fraction is 20% is added into suspension slurry
Solution adjusts the pH value of suspension slurry to 5~6, is heated to 50~60 DEG C, keeps the temperature 10~15h, obtain mixed serum;It will
Sieve sieving through 400 mesh after bentonite grinding, then through 600~800 DEG C of 2~4h of high-temperature calcination, light-burned bentonite is obtained,
20~30 parts of diatomite, 10~15 parts of light-burned bentonites are mixed, 400~500 mesh sieve is crossed, obtains mixed clay;By 35~50
Part nanometer titanium dioxide silica aerogel, 30~40 parts of above-mentioned mixed clays, 200~300 parts of water are mixed to get nano silicon dioxide gas
Mixed serum, nanometer titanium dioxide silica aerogel slurries are 4 by volume by gel slurries:1 mixing, is heated to 700~800 DEG C,
Melting feed liquid is obtained, modified alumina silicate fibre is obtained through spinning;150~200mL methyl-silicone oils are taken to be added with thermometer and return
In the three-necked flask for flowing device, three-necked flask is moved into sand-bath pot under nitrogen protection, control sand-bath temperature is 420~430
DEG C, after 1~2h of insulation reaction, 460~480 DEG C are warming up to, continues 40~50min of insulation reaction, after reaction natural cooling
To room temperature, product is obtained;200~300mL dimethylbenzene is added into above-mentioned product, filters, obtains after being stirred 10~15min
Filtrate is transferred in Rotary Evaporators by filtrate, and 40~50min of concentrated by rotary evaporation, obtains concentrate at 80~90 DEG C, take 30~
40g zirconium borides are added in pulverizer 30~40min of crushing, obtain boronation zirconium powder, by boronation zirconium powder, concentrate, 100~
200mL deionized waters are added in beaker, after being stirred 15~20min, obtain bonding agent;It counts in parts by weight, by 40~50
Part white fused alumina, 30~40 parts of obsidians, 20~25 parts of expansible graphites be added in pulverizer be crushed to particle diameter be 1~
It is poured into sand mixer after 3mm, then 10~15 parts of alumina powders, 0.3~0.5 part of Sodium Polyacrylate, 3~5 is added into sand mixer
Part zirconium dioxide, 5~8 parts of graphenes, are stirred 10~20min, sequentially add 8~10 parts of bonding agents and 20~25 parts change
Property alumina silicate fibre, continue to be stirred 5~10min, obtain mixing building stones, mixing building stones are tangled with modified alumina silicate fibre
Cladding is fitted into mold, 30~35min of hot pressing, and control hot pressing pressure is 10~20MPa, and hot pressing temperature is 200~300 DEG C, is obtained
To expansion heat insulation type fire proofing material.
Example 1
It counts in parts by weight, 70 parts of kaolin, 20 parts of aluminium oxide, 10 parts of titanium dioxides, 20 parts of aluminum phosphates is added into 400 parts of water,
It is dispersed with stirring and suspension slurry is made, the pH that the phosphoric acid solution that mass fraction is 20% adjusts suspension slurry is added into suspension slurry
Value is heated to 50 DEG C to 5, keeps the temperature 10h, obtains mixed serum;Sieve sieving through 400 mesh after bentonite is ground, then
Through 600 DEG C of high-temperature calcination 2h, light-burned bentonite is obtained, 20 parts of diatomite, 10 parts of light-burned bentonites are mixed, 400 mesh are crossed
Sieve, obtains mixed clay;35 parts of nanometer titanium dioxide silica aerogels, 30 parts of above-mentioned mixed clays, 200 parts of water are mixed to get nanometer
Mixed serum, nanometer titanium dioxide silica aerogel slurries are 4 by volume by aerosil slurries:1 mixing, is heated to
700 DEG C, melting feed liquid is obtained, modified alumina silicate fibre is obtained through spinning;150mL methyl-silicone oils are taken to be added with thermometer and return
In the three-necked flask for flowing device, three-necked flask is moved into sand-bath pot under nitrogen protection, control sand-bath temperature is 420 DEG C, is protected
After temperature reaction 1h, 460 DEG C are warming up to, continues insulation reaction 40min, cooled to room temperature, obtains product after reaction;To
200mL dimethylbenzene is added in above-mentioned product, is filtered after being stirred 10min, obtains filtrate, filtrate is transferred to Rotary Evaporators
In, concentrated by rotary evaporation 40min, obtains concentrate at 80 DEG C, takes 30g zirconium borides to be added in pulverizer and crushes 30min, obtains boron
Change zirconium powder, boronation zirconium powder, concentrate, 100mL deionized waters are added in beaker, after being stirred 15min, in conjunction with
Agent;It counts in parts by weight, 40 parts of white fused aluminas, 30 parts of obsidians, 20 parts of expansible graphites is added in pulverizer and are crushed to
Poured into sand mixer after a diameter of 1mm of grain, then be added into sand mixer 10 parts of alumina powders, 0.3 part of Sodium Polyacrylate, 3 part two
Zirconium oxide, 5 parts of graphenes, are stirred 10min, sequentially add 8 parts of bonding agents and 20 parts of modified alumina silicate fibres, continue to stir
Mixing 5min is mixed, obtains mixing building stones, mixing building stones are tangled to coat with modified alumina silicate fibre to be fitted into mold, hot pressing
30min, control hot pressing pressure are 10MPa, and hot pressing temperature is 200 DEG C, obtain expansion heat insulation type fire proofing material.
Example 2
It counts in parts by weight, 75 parts of kaolin, 25 parts of aluminium oxide, 12 parts of titanium dioxides, 21 parts of aluminum phosphates is added into 450 parts of water,
It is dispersed with stirring and suspension slurry is made, the pH that the phosphoric acid solution that mass fraction is 20% adjusts suspension slurry is added into suspension slurry
Value is heated to 55 DEG C to 5, keeps the temperature 12h, obtains mixed serum;Sieve sieving through 400 mesh after bentonite is ground, then
Through 700 DEG C of high-temperature calcination 3h, light-burned bentonite is obtained, 25 parts of diatomite, 12 parts of light-burned bentonites are mixed, 450 mesh sieve is crossed,
Obtain mixed clay;40 parts of nanometer titanium dioxide silica aerogels, 35 parts of above-mentioned mixed clays, 250 parts of water are mixed to get nanometer two
Mixed serum, nanometer titanium dioxide silica aerogel slurries are 4 by volume by silica aerogel slurries:1 mixing, is heated to 750
DEG C, melting feed liquid is obtained, modified alumina silicate fibre is obtained through spinning;It takes 175mL methyl-silicone oils to be added and carries thermometer and reflux
In the three-necked flask of device, three-necked flask is moved into sand-bath pot under nitrogen protection, control sand-bath temperature is 425 DEG C, heat preservation
After reacting 1.5h, 470 DEG C are warming up to, continues insulation reaction 45min, cooled to room temperature, obtains product after reaction;To
250mL dimethylbenzene is added in above-mentioned product, is filtered after being stirred 12min, obtains filtrate, filtrate is transferred to Rotary Evaporators
In, concentrated by rotary evaporation 45min, obtains concentrate at 85 DEG C, takes 30~40g zirconium borides to be added in pulverizer and crushes 35min, obtains
To boronation zirconium powder, boronation zirconium powder, concentrate, 100~200mL deionized waters are added in beaker, 17min is stirred
Afterwards, bonding agent is obtained;It counts in parts by weight, 45 parts of white fused aluminas, 35 parts of obsidians, 22 parts of expansible graphites is added to pulverizer
In be crushed to particle diameter be 2mm after pour into sand mixer, then into sand mixer be added 12 parts of alumina powders, 0.4 part of polypropylene
Sour sodium, 4 parts of zirconium dioxides, 7 parts of graphenes, are stirred 15min, sequentially add 9 parts of bonding agents and 22 parts of modified alumina silicate
Fiber continues to be stirred 8min, obtains mixing building stones, and the modified alumina silicate fibre entanglement cladding of mixing building stones is packed into mold
In, hot pressing 32min, control hot pressing pressure is 15MPa, and hot pressing temperature is 250 DEG C, obtains expansion heat insulation type fire proofing material.
Example 3
It counts in parts by weight, 80 parts of kaolin, 30 parts of aluminium oxide, 15 parts of titanium dioxides, 22 parts of aluminum phosphates is added into 500 parts of water,
It is dispersed with stirring and suspension slurry is made, the pH that the phosphoric acid solution that mass fraction is 20% adjusts suspension slurry is added into suspension slurry
Value is heated to 60 DEG C to 6, keeps the temperature 15h, obtains mixed serum;Sieve sieving through 400 mesh after bentonite is ground, then
Through 800 DEG C of high-temperature calcination 4h, light-burned bentonite is obtained, 30 parts of diatomite, 15 parts of light-burned bentonites are mixed, 500 mesh are crossed
Sieve, obtains mixed clay;50 parts of nanometer titanium dioxide silica aerogels, 40 parts of above-mentioned mixed clays, 300 parts of water are mixed to get nanometer
Mixed serum, nanometer titanium dioxide silica aerogel slurries are 4 by volume by aerosil slurries:1 mixing, is heated to
800 DEG C, melting feed liquid is obtained, modified alumina silicate fibre is obtained through spinning;200mL methyl-silicone oils are taken to be added with thermometer and return
In the three-necked flask for flowing device, three-necked flask is moved into sand-bath pot under nitrogen protection, control sand-bath temperature is 430 DEG C, is protected
After temperature reaction 2h, 480 DEG C are warming up to, continues insulation reaction 50min, cooled to room temperature, obtains product after reaction;To
300mL dimethylbenzene is added in above-mentioned product, is filtered after being stirred 15min, obtains filtrate, filtrate is transferred to Rotary Evaporators
In, concentrated by rotary evaporation 50min, obtains concentrate at 90 DEG C, takes 40g zirconium borides to be added in pulverizer and crushes 40min, obtains boron
Change zirconium powder, boronation zirconium powder, concentrate, 200mL deionized waters are added in beaker, after being stirred 20min, in conjunction with
Agent;It counts in parts by weight, 50 parts of white fused aluminas, 40 parts of obsidians, 25 parts of expansible graphites is added in pulverizer and are crushed to
Poured into sand mixer after a diameter of 3mm of grain, then be added into sand mixer 15 parts of alumina powders, 0.5 part of Sodium Polyacrylate, 5 part two
Zirconium oxide, 8 parts of graphenes, are stirred 20min, sequentially add 10 parts of bonding agents and 25 parts of modified alumina silicate fibres, continue
It is stirred 10min, obtains mixing building stones, the modified alumina silicate fibre entanglement cladding of mixing building stones is fitted into mold, hot pressing
35min, control hot pressing pressure are 20MPa, and hot pressing temperature is 300 DEG C, obtain expansion heat insulation type fire proofing material.
Comparative example
With the expansion heat insulation type fire proofing material of company of Hejian City production as a comparison case to expansion heat insulation type produced by the present invention
Expansion heat insulation type fire proofing material in fire proofing material and comparative example carries out performance detection, and testing result is as shown in table 1:
Test method:
Fire endurance time test:Fire proofing material in example 1~3 and comparative example is positioned at open fire, each fire proofing wood is recorded
Expect the time after having burnt;
Expansion multiplying power test is detected using expansion multiplying power tester;
Intensity test is detected by 161 standards of GA;
Flame retardant rating test is by flame retardant rating by HB, and incremental standard is detected step by step to V-0 by V-2, V-1.
1 fire proofing material performance measurement result of table
Good according to the expansion heat insulation type fire proofing material refractory heat-insulating performance produced by the present invention of data among the above, fire endurance reaches
To 78min, expansion multiplying power is high under the high temperature conditions, and compression strength is high upon inflation, has broad application prospects.
Claims (7)
1. a kind of preparation method of expansion heat insulation type fire proofing material, it is characterised in that specifically preparation process is:
(1)It counts in parts by weight, 70~80 parts of kaolin, 20~30 parts of aluminium oxide, 10~15 is added into 400~500 parts of water
Part titanium dioxide, 20~22 parts of aluminum phosphates, are dispersed with stirring and suspension slurry are made, and phosphoric acid solution is added into suspension slurry and adjusts suspension
The pH of slurries, heat temperature raising, heat preservation obtain mixed serum;
(2)It is sieved after bentonite is ground, high-temperature calcination obtains light-burned bentonite, by 20~30 parts of diatomite, 10~15 parts light
Bentonite mixing is burnt, sieving obtains mixed clay;
(3)35~50 parts of nanometer titanium dioxide silica aerogels, 30~40 parts of above-mentioned mixed clays, 200~300 parts of water are mixed to get
Nanometer titanium dioxide silica aerogel slurries mix mixed serum, nanometer titanium dioxide silica aerogel slurries, and heating obtains melting charge
Liquid obtains modified alumina silicate fibre through spinning;
(4)150~200mL methyl-silicone oils are taken to be added in the three-necked flask with thermometer and reflux, under nitrogen protection
Three-necked flask is moved into sand-bath pot, after insulation reaction, heating continues insulation reaction, after reaction cooled to room temperature,
Obtain product;
(5)200~300mL dimethylbenzene is added into above-mentioned product, is filtered after being stirred, obtains filtrate, filtrate is transferred to rotation
Turn in evaporimeter, concentrated by rotary evaporation obtains concentrate, takes 30~40g zirconium borides to be added in pulverizer and crushes, obtains boronation zirconium powder
Boronation zirconium powder, concentrate, 100~200mL deionized waters are added in beaker, after being stirred, obtain bonding agent by end;
(6)It counts in parts by weight, 40~50 parts of white fused aluminas, 30~40 parts of obsidians, 20~25 parts of expansible graphites is added to
It is poured into sand mixer after being crushed in pulverizer, then 10~15 parts of alumina powders, 0.3~0.5 part of polypropylene is added into sand mixer
Sour sodium, 3~5 parts of zirconium dioxides, 5~8 parts of graphenes, are stirred, and sequentially add 8~10 parts of bonding agents and 20~25 parts change
Property alumina silicate fibre, continue to be stirred, obtain mixing building stones, mixing building stones are packed into modified alumina silicate fibre cladding of tangling
In mold, hot pressing obtains expansion heat insulation type fire proofing material.
2. a kind of preparation method of expansion heat insulation type fire proofing material according to claim 1, it is characterised in that:Step(1)
The mass fraction of the phosphoric acid solution is 20%, and the pH value for adjusting suspension slurry is 5~6, after heat temperature raising temperature be 50~
60 DEG C, soaking time is 10~15h.
3. a kind of preparation method of expansion heat insulation type fire proofing material according to claim 1, it is characterised in that:Step(2)
It is 400 mesh that the bentonite, which grinds be sieved specification, and high-temperature calcination temperature is 600~800 DEG C, and calcination time is 2~4h, institute
Sieving specification is 400~500 mesh.
4. a kind of preparation method of expansion heat insulation type fire proofing material according to claim 1, it is characterised in that:Step(3)
The mixed serum, nanometer titanium dioxide silica aerogel slurries mixed volume ratio are 4:1, temperature is 700~800 after heat temperature raising
℃。
5. a kind of preparation method of expansion heat insulation type fire proofing material according to claim 1, it is characterised in that:Step(4)
The control sand-bath temperature is 420~430 DEG C, and the insulation reaction time is 1~2h, and temperature is 460~480 DEG C after heating, after
The continuation of insurance warm reaction time is 40~50min.
6. a kind of preparation method of expansion heat insulation type fire proofing material according to claim 1, it is characterised in that:Step(5)
The time that is stirred is 10~15min, and concentrated by rotary evaporation temperature is 80~90 DEG C, and the concentrated by rotary evaporation time is 40~50min,
It is 30~40min that zirconium boride, which is added to grinding time in pulverizer, and it is 15~20min to be stirred the time.
7. a kind of preparation method of expansion heat insulation type fire proofing material according to claim 1, it is characterised in that:Step(6)
Grain diameter is 1~3mm after the crushing, and it is 10~20min to be stirred the time, continue to be stirred the time be 5~
10min, hot pressing time are 30~35min, and control hot pressing pressure is 10~20MPa, and hot pressing temperature is 200~300 DEG C.
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CN109133723A (en) * | 2018-09-20 | 2019-01-04 | 黄勇 | A kind of preparation method of the heat-insulated carbon cloth of high temperature resistance to compression |
CN109208324A (en) * | 2018-09-20 | 2019-01-15 | 方建波 | A kind of preparation method of interior expansion nano hole heat-insulating material |
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CN110003542A (en) * | 2019-02-28 | 2019-07-12 | 常州苏通海平机电科技有限公司 | A kind of preparation method of heat-resistant anticorrosive rubber tube |
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CN111234537A (en) * | 2020-02-24 | 2020-06-05 | 哈尔滨理工大学 | Graphene anti-dripping flame-retardant synergist and preparation method thereof |
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